X-RAY DIFFRACTION

ARIF MAMUN AZAD

ROLL NO – CHM165046
YEAR- 3rd
SEMESTER-6th
CODE –PS 332
ALIAH UNIVERSITY, KOLKATA,160
What are X-rays ?
Generation Of X-rays :

When a free electron is

collided with a heavy
atom(Mo, W, Cu, Al etc)
it knocks an electron
of the lower orbital of the
atom ;an electron from its
higher orbital immediately
falls to the lower orbital to
fill the gap releasing an
extra energy as an
X-ray photon
Production of X-rays :

 X-rays are produced experimentally when high speed electrons

are collided with a metal target (generally Mo, W, Cu, Al)

 A source of electron is hot W filament; a high accelerating voltage

(~10k eV) between cathode(W) and anode and a metal target .

 Anode is a water cooled block of Cu containing desired target

metal .
What is X-ray diffraction
The most convenient and widely used method to determine the structural
properties of solid crystals

Types of X-ray related spectroscopies:-

 (i) X-ray absorbance
 (ii) X-ray diffraction
 (iii) X-ray fluorescence
 Every crystalline substance gives a pattern, same for the substance and
mixture of substances each produces its pattern independently .
 Therefore XRD pattern is like a fingerprint of substance . It`s based on
scattering of X-rays by crystals .
 Definition:- The atomic planes of a crystal cause an incident X-ray beam to
interfere one another .This phenomenon is called X-ray diffraction .
Why XRD ?

 A novel, non destructive, cheapest, in situ method

Measures the average spacing between the layer or rows of atoms

 Determines the orientation of a single crystal an d also polycrystals

or grains
 Measure the size, shape and internal stress of smaller crystalline
regions
 Modern X-ray
diffractometer
 Sample preparation
Powders

 0.1um < particle size < 40um

(Peak broadening) (Less diffraction occurring)

 Bulks:- smooth surface after polishing specimen should

be thermally annealed eliminate any surface
deformation induced during polishing
Bragg`s law
Detection of diffracted X-ray
on photographic plate :

 A sample of some hundred crystals (i.e.

powdered sample) show that the
diffracted beam from continuous cones .
A circle of films is used to record the
diffracted pattern as shown .

 Each cone intersects the film giving

diffracted lines . The lines are seen ass
arcs on the film
Basics of crystallography

 The atoms are arranged in a regular pattern and

there`s as smallest volume element that by
repetition in 3D describes the crystal . The
smallest volume element is called a unit cell .

 Crystals consist of atoms that are spaced a

distance apart, but can be resolved into many
atomic planes, each with a different spacing .

 The dimensions of the unit cell is described by 3

axes a,b,c and angles between them is A,B,C
and are lattice constants which can be
determined using XRD .
 Miller Indices :

 The LCM multiplied to the reciprocals of the fractional intercepts which the plane
makes with crystallographic axes .

 The axial length

 Intercepts

 Miller indices
 XRD methods
Laue method Rotating crystal method Debye Scherer
(powder method)

Orientation Lattice constant Lattice parameter

Single Crystal Single Crystal Polycrystal
Polychromatic beam Monochromatic beam Monochromatic beam

Fixed angle Variable angle Variable angle

 Applications of XRD
(i) Determination of the structure of the crystalline materials .
(ii) Determination of electron distribution within atom throughout the
cell .
(iii) Determination of orientation of single crystals .
(iv) Diffractions improved by computer technologies used to determine
the atomic structure and in various medical application like drug,
biomolecules structure elucidation and their working function to
living cells .
Disadvantage:- X-rays do not interact strongly with lighter
elements so as C-H bonds . So X-rays can`t determine the protein
structures .